CN103923083A - Adenine synthesis technology - Google Patents
Adenine synthesis technology Download PDFInfo
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- CN103923083A CN103923083A CN201410189028.4A CN201410189028A CN103923083A CN 103923083 A CN103923083 A CN 103923083A CN 201410189028 A CN201410189028 A CN 201410189028A CN 103923083 A CN103923083 A CN 103923083A
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- Prior art keywords
- acetyl
- vitamin
- weight parts
- ribose
- tetra
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 10
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 title abstract description 12
- 229930024421 Adenine Natural products 0.000 title abstract description 12
- 229960000643 adenine Drugs 0.000 title abstract 11
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 51
- OIRDTQYFTABQOQ-KQYNXXCUSA-N adenosine Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O OIRDTQYFTABQOQ-KQYNXXCUSA-N 0.000 claims abstract description 30
- 239000002126 C01EB10 - Adenosine Substances 0.000 claims abstract description 15
- 229960005305 adenosine Drugs 0.000 claims abstract description 15
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 3
- 235000013343 vitamin Nutrition 0.000 claims description 52
- 239000011782 vitamin Substances 0.000 claims description 52
- 229940088594 vitamin Drugs 0.000 claims description 52
- 229930003231 vitamin Natural products 0.000 claims description 52
- 150000003722 vitamin derivatives Chemical class 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000009413 insulation Methods 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 22
- -1 acetyl VITAMIN Chemical class 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000002425 crystallisation Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 10
- 239000006188 syrup Substances 0.000 claims description 10
- 235000020357 syrup Nutrition 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 6
- 235000008504 concentrate Nutrition 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- IHNHAHWGVLXCCI-FDYHWXHSSA-N [(2r,3r,4r,5s)-3,4,5-triacetyloxyoxolan-2-yl]methyl acetate Chemical compound CC(=O)OC[C@H]1O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H]1OC(C)=O IHNHAHWGVLXCCI-FDYHWXHSSA-N 0.000 abstract 1
- 230000000397 acetylating effect Effects 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 4
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- LTMRRSWNXVJMBA-UHFFFAOYSA-L 2,2-diethylpropanedioate Chemical compound CCC(CC)(C([O-])=O)C([O-])=O LTMRRSWNXVJMBA-UHFFFAOYSA-L 0.000 description 1
- 238000004176 ammonification Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000003212 purines Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 235000008979 vitamin B4 Nutrition 0.000 description 1
- 239000011579 vitamin B4 Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D473/00—Heterocyclic compounds containing purine ring systems
- C07D473/26—Heterocyclic compounds containing purine ring systems with an oxygen, sulphur, or nitrogen atom directly attached in position 2 or 6, but not in both
- C07D473/32—Nitrogen atom
- C07D473/34—Nitrogen atom attached in position 6, e.g. adenine
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention discloses an adenine synthesis technology. The adenine synthesis technology comprises the following steps: acetylating adenosine serving as a substrate by using acetic anhydride so as to obtain acetylated adenine and tetraacetylribose, carrying out alkaline hydrolysis on the acetylated adenine, and neutralizing the acetylated adenine so as to obtain adenine. The adenine synthesis technology is simple, very beneficial to the large-scale production of the adenine and capable of greatly reducing the processing cost of the adenine and improving the production efficiency of the adenine.
Description
Technical field:
The present invention relates to the manufacture of VITAMIN B4, particularly a kind of VITAMIN B4 synthesis technique.
Background technology:
VITAMIN B4, chemistry 6-aminopurine by name, is the main raw material of synthesise vitamins B4, every year domestic also have hundreds of tons of VITAMIN B4 outlets to sell to world market for preparing the medicines such as purines derivative.Except the complete synthesizing process by diethyl malonate makes, the technique of domestic manufacturer's suitability for industrialized production VITAMIN B4 is all to take xanthoglobulin as starting raw material at present, with phosphorus oxychloride, N, N-xylidine reacts synthetic through chlorination, hydrolysis, pressurization ammonification, refine etc., reactions steps is many, and yield is low, disposal of three wastes amount is large.
Summary of the invention:
The object of this invention is to provide the VITAMIN B4 synthesis technique that a kind of technique is simple, be beneficial to large-scale production.
Technical scheme of the present invention is, a VITAMIN B4 synthesis technique, is characterized in that: it comprises following production stage: (1) first adds the aceticanhydride measuring in dry reactor, opens and stirs simultaneously, slowly drop into adenosine, with chuck, be heated to 110 ℃, utilize the remaining temperature of chuck that adenosine is dissolved, molten clear after, add boric acid, 110 ℃ of-115 ℃ of insulation reaction, after about 1.5-2.5 hour, reaction solution is muddy gradually, continues 110 ℃ of-115 ℃ of insulation reaction and lowers the temperature and spend the night after 10 hours; (2) above-mentioned reaction solution suction filtration is separated, filter cake is acetyl VITAMIN B4, standby after drying; (3) mother liquor in step (2) concentrates acetic acid and aceticanhydride mixed solution to dry by negative pressure, and the syrup obtaining washes with water, decrease temperature crystalline, obtains crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose; (4) crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose is dissolved by industrial methanol, activated carbon decolorizing, and after filtering, crystallisation by cooling spends the night; (5) 1,2,3,5-Tetra-O-Acetyl-D-Ribose of advantages of good crystallization is obtained to 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product by centrifugation, 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product is dropped into 70～75 ℃ of oven dry in double-cone dryer, dry the 1,2,3,5-Tetra-O-Acetyl-D-Ribose that arrives of rear packing; (6) by the water suction reactor measuring, open and stir, the sodium hydroxide that adds specified amount, after finishing, slowly the acetyl VITAMIN B4 that obtains measuring is dropped into reactor in step (2), after the end that feeds intake, be warming up to 60 ℃, after acetyl VITAMIN B4 is all dissolved, add gac, continue 60 ℃ of insulation decolourings 1 hour, filtering separation gac; (7), after filtering, mother liquor continues to be warming up to 90 ℃ of insulation alkaline hydrolysis and after 2 hours, is cooled to 40 ℃, starts to be neutralized to neutrality with hydrochloric acid, separates out VITAMIN B4; (8) after neutralization finishes, cooling is spent the night; The centrifugal VITAMIN B4 wet product that obtains; (9) VITAMIN B4 wet product completes preparation after drying.The consumption of each described reaction substrate is counted by weight: adenosine: 38～40 weight parts, aceticanhydride: 110～120 weight parts, boric acid: 2.5～3.5 weight parts, industrial methanol: 100～110 weight parts, water (in step 3): 100～110 weight parts, water (in step 6): 300～350 weight parts, sodium hydroxide: 15～25 weight parts, gac (in step 4): 1～3 weight part, gac (in step 6): 1～3 weight part, hydrochloric acid: 8～12 weight parts.
Technique of the present invention is simple, is beneficial to very much the large-scale production of VITAMIN B4, can reduce greatly the tooling cost of VITAMIN B4, has improved the production efficiency of VITAMIN B4.
Embodiment:
Describe embodiments of the invention in detail,
Embodiment 1,
First the aceticanhydride of 110 weight parts that measure is added in dry reactor, open and stir simultaneously, slowly drop into the adenosine of 38 weight parts, with chuck, be heated to 110 ℃, utilize the remaining temperature of chuck that adenosine is dissolved, molten clear after, the boric acid that adds 2.5 weight parts, 110 ℃ of insulation reaction, after 1.5 hours, reaction solution is muddy gradually, continues 110 ℃ of insulation reaction and lowers the temperature and spend the night after 10 hours; (2) above-mentioned reaction solution suction filtration is separated, filter cake is acetyl VITAMIN B4, standby after drying; (3) mother liquor in step (2) concentrates acetic acid and aceticanhydride mixed solution to dry by negative pressure, the syrup obtaining, in preprepared reactor, add after 100 weight parts waters that measure in syrup suction still, wash, be cooled to 20 ℃ of crystallizations with water, after filtration, obtain crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose; (4) the crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose in step 3 is dissolved by the industrial methanol of 100 weight parts, and with the activated carbon decolorizing of 1 weight part, after filtering, crystallisation by cooling spends the night; (5) 1,2,3,5-Tetra-O-Acetyl-D-Ribose of advantages of good crystallization is obtained to 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product by centrifugation, 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product is dropped into double-cone dryer and at 70 ℃, dry, dry the 1,2,3,5-Tetra-O-Acetyl-D-Ribose that arrives of rear packing; (6) by the water suction reactor of 300 weight parts that measure, open and stir, the sodium hydroxide that adds 15 weight parts, after finishing, slowly the acetyl VITAMIN B4 that obtains measuring is dropped into reactor in step (2), after the end that feeds intake, be warming up to 60 ℃, after acetyl VITAMIN B4 is all dissolved, add 1 weight part gac, continue 60 ℃ of insulation decolourings 1 hour, filtering separation gac; (7), after filtering, mother liquor continues to be warming up to 90 ℃ of insulation alkaline hydrolysis and after 2 hours, is cooled to 40 ℃, starts to be neutralized to neutrality with the hydrochloric acid of 8 weight parts, separates out VITAMIN B4; (8) after neutralization finishes, cooling is spent the night; The centrifugal VITAMIN B4 wet product that obtains; (9) VITAMIN B4 wet product completes preparation after drying at 110 ℃.
Embodiment 2,
First the aceticanhydride of 115 weight parts that measure is added in dry reactor, open and stir simultaneously, slowly drop into the adenosine of 39 weight parts, with chuck, be heated to 110 ℃, utilize the remaining temperature of chuck that adenosine is dissolved, molten clear after, the boric acid that adds 3 weight parts, 115 ℃ of insulation reaction, after 2 hours, reaction solution is muddy gradually, continues 115 ℃ of insulation reaction and lowers the temperature and spend the night after 10 hours; (2) above-mentioned reaction solution suction filtration is separated, filter cake is acetyl VITAMIN B4, standby after drying; (3) mother liquor in step (2) concentrates acetic acid and aceticanhydride mixed solution to dry by negative pressure, the syrup obtaining, in preprepared reactor, add after 105 weight parts waters that measure in syrup suction still, wash, be cooled to 20 ℃ of crystallizations with water, after filtration, obtain crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose; (4) the crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose in step 3 is dissolved by the industrial methanol of 105 weight parts, and with the activated carbon decolorizing of 2 weight parts, after filtering, crystallisation by cooling spends the night; (5) 1,2,3,5-Tetra-O-Acetyl-D-Ribose of advantages of good crystallization is obtained to 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product by centrifugation, 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product is dropped into double-cone dryer and at 73 ℃, dry, dry the 1,2,3,5-Tetra-O-Acetyl-D-Ribose that arrives of rear packing; (6) by the water suction reactor of 320 weight parts that measure, open and stir, the sodium hydroxide that adds 25 weight parts, after finishing, slowly the acetyl VITAMIN B4 that obtains measuring is dropped into reactor in step (2), after the end that feeds intake, be warming up to 60 ℃, after acetyl VITAMIN B4 is all dissolved, add 2 weight part gacs, continue 60 ℃ of insulation decolourings 1 hour, filtering separation gac; (7), after filtering, mother liquor continues to be warming up to 90 ℃ of insulation alkaline hydrolysis and after 2 hours, is cooled to 40 ℃, starts to be neutralized to neutrality with the hydrochloric acid of 10 weight parts, separates out VITAMIN B4; (8) after neutralization finishes, cooling is spent the night; The centrifugal VITAMIN B4 wet product that obtains; (9) VITAMIN B4 wet product completes preparation after drying at 110 ℃.
Embodiment 3,
First the aceticanhydride of 120 weight parts that measure is added in dry reactor, open and stir simultaneously, slowly drop into the adenosine of 40 weight parts, with chuck, be heated to 110 ℃, utilize the remaining temperature of chuck that adenosine is dissolved, molten clear after, the boric acid that adds 3.5 weight parts, 113 ℃ of insulation reaction, after 2.5 hours, reaction solution is muddy gradually, continues 112 ℃ of insulation reaction and lowers the temperature and spend the night after 10 hours; (2) above-mentioned reaction solution suction filtration is separated, filter cake is acetyl VITAMIN B4, standby after drying; (3) mother liquor in step (2) concentrates acetic acid and aceticanhydride mixed solution to dry by negative pressure, the syrup obtaining, in preprepared reactor, add after 110 weight parts waters that measure in syrup suction still, wash, be cooled to 20 ℃ of crystallizations with water, after filtration, obtain crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose; (4) the crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose in step 3 is dissolved by the industrial methanol of 110 weight parts, and with the activated carbon decolorizing of 3 weight parts, after filtering, crystallisation by cooling spends the night; (5) 1,2,3,5-Tetra-O-Acetyl-D-Ribose of advantages of good crystallization is obtained to 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product by centrifugation, 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product is dropped into double-cone dryer and at 75 ℃, dry, dry the 1,2,3,5-Tetra-O-Acetyl-D-Ribose that arrives of rear packing; (6) by the water suction reactor of 350 weight parts that measure, open and stir, the sodium hydroxide that adds 20 weight parts, after finishing, slowly the acetyl VITAMIN B4 that obtains measuring is dropped into reactor in step (2), after the end that feeds intake, be warming up to 60 ℃, after acetyl VITAMIN B4 is all dissolved, add 3 weight part gacs, continue 60 ℃ of insulation decolourings 1 hour, filtering separation gac; (7), after filtering, mother liquor continues to be warming up to 90 ℃ of insulation alkaline hydrolysis and after 2 hours, is cooled to 40 ℃, starts to be neutralized to neutrality with the hydrochloric acid of 12 weight parts, separates out VITAMIN B4; (8) after neutralization finishes, cooling is spent the night; The centrifugal VITAMIN B4 wet product that obtains; (9) VITAMIN B4 wet product completes preparation after drying at 110 ℃.
Embodiment 4,
First the aceticanhydride of 118 weight parts that measure is added in dry reactor, open and stir simultaneously, slowly drop into the adenosine of 39 weight parts, with chuck, be heated to 110 ℃, utilize the remaining temperature of chuck that adenosine is dissolved, molten clear after, the boric acid that adds 3 weight parts, 111 ℃ of insulation reaction, after 2 hours, reaction solution is muddy gradually, continues 110 ℃ of insulation reaction and lowers the temperature and spend the night after 10 hours; (2) above-mentioned reaction solution suction filtration is separated, filter cake is acetyl VITAMIN B4, standby after drying; (3) mother liquor in step (2) concentrates acetic acid and aceticanhydride mixed solution to dry by negative pressure, the syrup obtaining, in preprepared reactor, add after 108 weight parts waters that measure in syrup suction still, wash, be cooled to 20 ℃ of crystallizations with water, after filtration, obtain crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose; (4) the crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose in step 3 is dissolved by the industrial methanol of 108 weight parts, and with the activated carbon decolorizing of 2.5 weight parts, after filtering, crystallisation by cooling spends the night; (5) 1,2,3,5-Tetra-O-Acetyl-D-Ribose of advantages of good crystallization is obtained to 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product by centrifugation, 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product is dropped into double-cone dryer and at 74 ℃, dry, dry the 1,2,3,5-Tetra-O-Acetyl-D-Ribose that arrives of rear packing; (6) by the water suction reactor of 328 weight parts that measure, open and stir, the sodium hydroxide that adds 22 weight parts, after finishing, slowly the acetyl VITAMIN B4 that obtains measuring is dropped into reactor in step (2), after the end that feeds intake, be warming up to 60 ℃, after acetyl VITAMIN B4 is all dissolved, add 2.8 weight part gacs, continue 60 ℃ of insulation decolourings 1 hour, filtering separation gac; (7), after filtering, mother liquor continues to be warming up to 90 ℃ of insulation alkaline hydrolysis and after 2 hours, is cooled to 40 ℃, starts to be neutralized to neutrality with the hydrochloric acid of 11 weight parts, separates out VITAMIN B4; (8) after neutralization finishes, cooling is spent the night; The centrifugal VITAMIN B4 wet product that obtains; (9) VITAMIN B4 wet product completes preparation after drying at 110 ℃.
Technique of the present invention is simple, is beneficial to very much the large-scale production of VITAMIN B4, can reduce greatly the tooling cost of VITAMIN B4, has improved the production efficiency of VITAMIN B4.
Claims (2)
1. a VITAMIN B4 synthesis technique, it is characterized in that: it comprises following production stage: (1) first adds the aceticanhydride measuring in dry reactor, open and stir simultaneously, slowly drop into adenosine, with chuck, be heated to 110 ℃, utilize the remaining temperature of chuck that adenosine is dissolved, molten clear after, add boric acid, 110 ℃ of-115 ℃ of insulation reaction, after about 1.5-2.5 hour, reaction solution is muddy gradually, continues 110 ℃ of-115 ℃ of insulation reaction and lowers the temperature and spend the night after 10 hours; (2) above-mentioned reaction solution suction filtration is separated, filter cake is acetyl VITAMIN B4, standby after drying; (3) mother liquor in step (2) concentrates acetic acid and aceticanhydride mixed solution to dry by negative pressure, and the syrup obtaining washes with water, decrease temperature crystalline, obtains crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose; (4) crude product 1,2,3,5-Tetra-O-Acetyl-D-Ribose is dissolved by industrial methanol, activated carbon decolorizing, and after filtering, crystallisation by cooling spends the night; (5) 1,2,3,5-Tetra-O-Acetyl-D-Ribose of advantages of good crystallization is obtained to 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product by centrifugation, 1,2,3,5-Tetra-O-Acetyl-D-Ribose wet product is dropped into 70～75 ℃ of oven dry in double-cone dryer, dry the 1,2,3,5-Tetra-O-Acetyl-D-Ribose that arrives of rear packing; (6) by the water suction reactor measuring, open and stir, the sodium hydroxide that adds specified amount, after finishing, slowly the acetyl VITAMIN B4 that obtains measuring is dropped into reactor in step (2), after the end that feeds intake, be warming up to 60 ℃, after acetyl VITAMIN B4 is all dissolved, add gac, continue 60 ℃ of insulation decolourings 1 hour, filtering separation gac; (7), after filtering, mother liquor continues to be warming up to 90 ℃ of insulation alkaline hydrolysis and after 2 hours, is cooled to 40 ℃, starts to be neutralized to neutrality with hydrochloric acid, separates out VITAMIN B4; (8) after neutralization finishes, cooling is spent the night; The centrifugal VITAMIN B4 wet product that obtains; (9) VITAMIN B4 wet product completes preparation after drying.
2. a kind of VITAMIN B4 synthesis technique as claimed in claim 1, it is characterized in that: the consumption of each described reaction substrate is counted by weight: adenosine: 38～40 weight parts, aceticanhydride: 110～120 weight parts, boric acid: 2.5～3.5 weight parts, industrial methanol: 100～110 weight parts, the add-on of water in step 3: 100～110 weight parts, the add-on of water in step 6: 300～350 weight parts, sodium hydroxide: 15～25 weight parts, the add-on of gac in step 4: 1～3 weight part, the add-on of gac in step 6: 1～3 weight part, hydrochloric acid: 8～12 weight parts.
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| CN201410189028.4A CN103923083A (en) | 2014-05-07 | 2014-05-07 | Adenine synthesis technology |
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| CN201410189028.4A CN103923083A (en) | 2014-05-07 | 2014-05-07 | Adenine synthesis technology |
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| CN105906629A (en) * | 2016-06-21 | 2016-08-31 | 宿迁远扬生物科技有限公司 | Technological process for synthesizing adenine |
| CN109575028A (en) * | 2018-12-21 | 2019-04-05 | 新乡医学院 | A method of adenosine is hydrolyzed using catalyzing cation exchange resin-separation coupling technology |
| CN111362945A (en) * | 2020-04-23 | 2020-07-03 | 洛阳德胜生物科技股份有限公司 | Method for synthesizing adenine by adenosine hydrolysis method |
| CN111410669A (en) * | 2019-01-04 | 2020-07-14 | 上海艾美晶生物科技有限公司 | Method for preparing D-ribose and base |
| CN111440170A (en) * | 2020-04-22 | 2020-07-24 | 通辽德胜生物科技有限公司 | Method for synthesizing guanine by using guanosine |
| CN111961056A (en) * | 2020-08-26 | 2020-11-20 | 通辽德胜生物科技有限公司 | Method for simultaneously synthesizing hypoxanthine and tetraacetyl ribose by utilizing inosine |
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2014
- 2014-05-07 CN CN201410189028.4A patent/CN103923083A/en active Pending
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906629A (en) * | 2016-06-21 | 2016-08-31 | 宿迁远扬生物科技有限公司 | Technological process for synthesizing adenine |
| CN109575028A (en) * | 2018-12-21 | 2019-04-05 | 新乡医学院 | A method of adenosine is hydrolyzed using catalyzing cation exchange resin-separation coupling technology |
| CN109575028B (en) * | 2018-12-21 | 2021-06-29 | 新乡医学院 | A kind of method that utilizes cation exchange resin catalysis-separation coupling technology to hydrolyze adenosine |
| CN111410669A (en) * | 2019-01-04 | 2020-07-14 | 上海艾美晶生物科技有限公司 | Method for preparing D-ribose and base |
| CN111440170A (en) * | 2020-04-22 | 2020-07-24 | 通辽德胜生物科技有限公司 | Method for synthesizing guanine by using guanosine |
| CN111440170B (en) * | 2020-04-22 | 2021-09-14 | 通辽德胜生物科技有限公司 | Method for synthesizing guanine by using guanosine |
| CN111362945A (en) * | 2020-04-23 | 2020-07-03 | 洛阳德胜生物科技股份有限公司 | Method for synthesizing adenine by adenosine hydrolysis method |
| CN111961056A (en) * | 2020-08-26 | 2020-11-20 | 通辽德胜生物科技有限公司 | Method for simultaneously synthesizing hypoxanthine and tetraacetyl ribose by utilizing inosine |
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